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5th December 2012 @ 03:52
Reaction Scheme PY14.png

DMF (5.0 mL) was stirred under a nitrogen atmosphere in an ice-bath. Phosphoryl chloride (1.18 mL, 12.7 mmol, 1.2 equiv.) was added and the reaction stirred for 25 minutes. A solution of pyrrole PMY 1-6 (2.00 g, 10.5 mmol, 1 equiv.) in DMF (5 mL) was added dropwise over 5 minutes. The reaction was removed from the ice-bath and allowed to warm to room temperature. After 1 h, reaction was complete by TLC. Poured over ice (100 ml). pH adjusted to 6 (approx. 10% NaOH) and left stirring overnight. In the morning pH was 1. 20% NaOH added until pH 11 and the reaction mixture was left to stir for a further 30 minutes. The mixture was filtered to give a beige paste that was recrystallised from MeCN/water to give a dark brown crystalline solid.
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